Halogenated composition



Patented Apr. 18, 1935 UNITED STATES iwiisu'rl OFFICE Malignant.acorner-stimo(NewYorkA Electr mm am um as, im. seria No.'m,s4s

sismici. :isz-1)"l l oeeurreo. ri has refractive index at 25 c.

The present invention comprises new hydrocarbon compositions which aresuitable. forl use as dielectric materials in transformers, capacitors.switches, cables, electric bushings, and other 5 forms of electricaldevices. Buch compositions may be used either alone or in conjunctionwith modifying ingredients. i

As described in prior U. S. Patents 1,931,373 and 1,931,455, bothpatented October 17, 1933, it is advantageous to employ in transformers,capacitors, switches and other electrical devices a dielectric materialcomprising one or more liquid halogenated hydrocarbons preferablyhydrocarbons containing a suillcient high proportionof halogen to rendernon-inflammable whatever gases may be evolved for any reason from auchdielectric. Heretofore only halogenated cyclic hydrocarbons, such forexample as chlorinated diphenyl or chlorinated benzene have been foundsumciently stable for this purpose. Aliphatic compounds, such as carbontetrachloride and chlorinated ethane have proven to be unsuitablebecause of chemical instability and corrosiveness` toward metal membersof electrical devices.

We have discovered that halogenated unsaturated oleiln compounds may becaused to polymerlze tov form new compositions and that such-compositions are suitable for luse as dielectric materials either bythemselves or in admixture with other insulating products.

The accompanying drawing is a graph showing the pour points of diiierentmixtures of lone of ournew products and trichlor benzene.

Trichlor ethylene is a mobile liquid boiling at 85 C. When this liquidis heated in contact with aluminum chloride polymerization occurs withthe formation of various polymerization products as will be described.When 30 mois of trichlor ethylene and 3 mols of aluminum chloride areheated in a reflux condenser at about y8!5C. a liquid polymerizationproduct is obtained having a boiling point o1' about 150 to 2209 C. Thispolymerization product when puriiled hyv filteringthrough fullers earthand sodium carbonate has a specific gravity of.. approximateLvLdZ.. Itlhas a dielectric constant stroom temperature of 3.25. and functionswith a powerfactor of approximate- 1y 2 per cent. The puriiled,polymerized product is chemically stable and is inert with respect tometals. For example, aluminum may be exposed a to such product either inliquid or vapor form at temperourres as man es io'o" c. without enemieeiaction taking place. when heatedunder pressurein a sealed-tube at 100"C. for 24 houx-'s in an atmosphere of nitrogen no. breakdown of theliquid of 1.5435to 1.5485. -Ithasapour pointor freezing point lower thanminus C. It has an acidity less than that neutralizable by .1 m. g. ofsodium hydroxide per gram. y o

When the heating in the rei'iux condenser of the above product iscontinued for a longer time there is formed a v more highly polymerizedproduct which is a'viscousseml-solidor a solid resin of dark redcoloration and also having physical and' chemical properties hrenderingit suitable for dielectric use. This'product is not distillable attemperaturesas high as 300 C. It is soluble in mineral oil. When thispolymerized product is desired we prefer to employ al larger proportionof aluminum chloride than in the case above given.- llior example, when2 mols of trichlor /ethylene and 1 mol of aluminum chloride are reiluxedat C., the liquid polymerization product above described is evolvedtogether with hydrogen chloride gas and upon continued heating theresinous -product above described is formed. At the end of about ilfteenminutes the polymerization will proceed as far as the formation of theliquid product. When the reiluxing is continued for about one hour thered resinous mass is obtained. Trichlor ethylene also maybe poly-vmerlzed by `passing its vapor through a tube product and '15% oftrichlorbenzene has a pom'- point of about minus 6 C. and a viscosityfofapproidmatelyf35`to 40 seconds. Trichlor benzene itself has a pour point'of about plus 10 C.,'a boiling point of 210 to 220 C., and a viscosityof vIn the is-sown'p. graph of pour points over a temperature range ofmixtures containing Y various percentages of trichlor-benzene and aresinous polymerization product, the temperature` being plotted asordinates and the precentage of 'resin as abscissae. A- eutectic mixturehaving a pour point of minus 45 C. is obtainedwhen the composition iscomposed of about equal parts trlevidenttrom the graph mixtures made upot about 25 to-75 per cent ot trichlor hemmene.` and of about 75 to 25percent oi the above-deeeribed resin have pour points, (that is, remainliquid), weil below 0 C.

Polymerized, lmsaturated, halogenated,l ali- -phatic hydrocarbons otherthan those prepared irom trichlorethylene come within the scope ot ourinvention. For example polymeriaed di-ior tetra hlogenated ethylene alsothe polymerised products of halogenated acetylene, propylene,

' butylene, and the like, may be prepared and employed for dielectricpurposes. Mixtures oi' the polymerized products with other halogenatedcompounds such, for example, as chlorinated dithe art that otherhaiosens such as uorine.

bromine and iodine may be substituted for the chlorine in thepolymerined, unsaturated, chlorinated, aliphatic hydrocarbons hereindescribed without departing from the spirit and scope of our invention.A

chlorbenrene snd trichlor ethylene resin. As is ILAresinousproductderivedbythcpobmer ization of trichlorethylene,saidproducthcin o! redcoloratiombcingsdubleinminenloilandresistingtemperaturessshichal'avithout distillaticn.

.2.Acompositionotmattercompriainamix ture oi trichlorbenmene and s solidresinous poiymemation product oi trichlor ethylene.

3. A composition of matter consisting ofsubstantiallytoopercentotasolidresinouspolymerizedtrichlorethyleneand'toper centottrichlor bensene,saidcomposition havin' aporpointatlcastasiowasmincandaviscositywithinthelimitsoiaboutto secondsaybolt.

4. A composition consisting essentially o( 2i to 75 per cent oftrichlorethyiene resin and 75 tomipercento!trichiorbexmeme,saidcomposi-vtion solidiiying atatemperaturebeiov 0 C.

5. A composition consisting of substcntialiy eqalpartsot trichlorethyleneresinlnd triehior benzene', said oompodtion remaininl liquid attemperatures sslow as minus 45 C.

FRANK H. CLARK. 'WALTER ILKUTZ.

